For quality control purpose,an approach of combining chromatographic fingerprint of Huaijiao pill（HP）and simultaneous determination of its major bioactive components was developed using high performance liquid chrom...For quality control purpose,an approach of combining chromatographic fingerprint of Huaijiao pill（HP）and simultaneous determination of its major bioactive components was developed using high performance liquid chromatography coupled with diode array detector（HPLC-DAD）.For fingerprint analysis,16 peaks were selected as the characteristic peaks to evaluate the similarities of different samples collected from different batches of three manufacturers.The similarities of 17 Huaijiao pill samples were beyond 0.966,indicating that samples from different batches and manufacturers were,to some extent,consistent.Additionally,simultaneous quantification of seven bioactive markers,namely sophoricoside,baicalin,naringin,genistein,rutin,quercetin and 5-O-methylvisammioside,in HP was performed to interpret the quality consistency.The validation of the proposed approach was acceptable,with the accuracy of 90.2%-106.9%in recovery test.The intra-day and inter-day precisions of the method were evaluated and the RSD values were less than 2.81%.The results from the quantitative data showed that the contents of six marker compounds（except for 5-O-methylvisammioside） were quite consistent between batches produced by one manufacturer and significantly distinctive among different manufacturers.The proposed approach was expected to be developed as a powerful tool for the quality control of HP.展开更多
Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chro...Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was considered as a reference compound and quantified.Relative standard deviations of retention time and peak area of each component were less than 3% and 8%,respectively.Similarity and difference analysis were conducted by use of PCA and relation coefficient.Twenty batches of sarcandra glabra(Thunb.)samples from two different producing areas could be classified into two different groups in the PCA model.The results showed that MAE-HPLC/DAD method was simple,efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra(Thunb.),which could provide more reliable and precise information for quality evaluation.展开更多
In this study, whole-oil gas chromatographic fingerprint analyses were performed on oils from the Es3^3 reservoir in the Liubei area of the Nanpu Sag. The gas chromatographic peaks of cyclic and branched alkanes with ...In this study, whole-oil gas chromatographic fingerprint analyses were performed on oils from the Es3^3 reservoir in the Liubei area of the Nanpu Sag. The gas chromatographic peaks of cyclic and branched alkanes with relatively high resolution from nCl0 to nC25 were selected to establish a database of whole-oil gas chromatographic peak height ratio fingerprints. Reservoir fluid connectivity was identified by using clustering analysis. This method can reflect the gas chromatography fingerprint information accurately and entirely, and avoid the one-sidedness of the star diagram method which only selects several fixed gas chromatographic peaks.展开更多
A simple and facile gas chromatography-mass spectrometer （GC-MS） fingerprint of Su-He-Xiang-Wan （SHXW） was developed, the similarity analysis was conducted, and attribution of the major characteristic peaks was id...A simple and facile gas chromatography-mass spectrometer （GC-MS） fingerprint of Su-He-Xiang-Wan （SHXW） was developed, the similarity analysis was conducted, and attribution of the major characteristic peaks was identified for SHXW quality control. GC-MS analysis was performed on a QP2010 instrument （Shimadzu, Japan） equipped with a capillary column of RTX-5MS. The column temperature was initiated at 50℃, held for 5 min, increased at the rate of 3 ℃/min to 120 ℃, held for 2 min, and then increased at the rate of 4 ℃/min to 220℃, held for 10 min. Helium carrier gas was used at a constant flow rate of 1.3 mL/min. Mass conditions were ionization voltage, 70 eV; injector temperature, 250℃; ion source temperature, 250 ℃; splitting ratio, 30：1; full scan mode in the 40-500 Da mass ranges with rate of 0.2 s per scan. Attribution of the major characteristic peaks was identified for SHXW by comparing the chemical standards, references of Chinese herbal medicines and the negative controls of prescription samples （NC） of SHXW. With the help of the temperature-programmed retention indices （PTRIs） used together with mass spectra and chemical standards, 25 major characteristic peaks have been identified. Nine volatile medicinal materials were identified in the prescription of SHXW by attributing to the 27 major characteristic peaks. The results demonstrate that the proposed method is a powerful approach to quality control of complex herbal medicines.展开更多
Objective To facilitate the quality evaluation suitable for the unique characteristics of Chinese materia medica(CMM)by developing and implementing a novel approach known as the matching frequency statistical moment(M...Objective To facilitate the quality evaluation suitable for the unique characteristics of Chinese materia medica(CMM)by developing and implementing a novel approach known as the matching frequency statistical moment(MFSM)method.Methods This study established the MFSM method.To demonstrate its effectiveness,we applied this novel approach to analyze Danxi Granules(丹膝颗粒,DXG)and its constituent herbal materials.To begin with,the ultra-performance liquid chromatography(UPLC)was applied to obtain the chromatographic fingerprints of DXG and its constituent herbal materi-als.Next,the MFSM was leveraged to compress and integrate them into a new fingerprint with fewer analytical units.Then,we characterized the properties and variability of both the original and integrated fingerprints by calculating total quantum statistical moment(TQSM)parameters,information entropy and information amount,along with their relative standard deviation(RSD).Finally,we compared the TQSM parameters,information entropy and infor-mation amount,and their RSD between the traditional and novel fingerprints to validate the new analytical method.Results The chromatographic peaks of DXG and its 12 raw herbal materials were divided and integrated into peak families by the MFSM method.Before integration,the ranges of the peak number,three TQSM parameters,information entropy and information amount for each peak or peak family of UPLC fingerprints of DXG and its 12 raw herbal materials were 95.07−209.73,9390−183064μv·s,5.928−21.33 min,22.62−106.69 min^(2),4.230−6.539,and 50530−974186μv·s,respectively.After integration,the ranges of these parameters were 10.00−88.00,9390−183064μv·s,5.951−22.02 min,22.27−104.73 min^(2),2.223−5.277,and 38159−807200μv·s,respectively.Correspondingly,the RSD of all the aforementioned pa-rameters before integration were 2.12%−9.15%,6.04%−49.78%,1.15%−23.10%,3.97%−25.79%,1.49%−19.86%,and 6.64%−51.20%,respectively.However,after integration,they changed to 0.00%,6.04%−49.87%,1.73%−23.02%,3.84%−26.85%,1.17%−16.54%,and 6.40%−48.59%,respectively.The results demonstrated that in the newly integrated fingerprint,the analytical units of constituent herbal materials,information entropy and information amount were significantly reduced(P<0.05),while the TQSM parameters remained unchanged(P>0.05).Additionally,the RSD of the TQSM parameters,information entropy,and information amount didn’t show significant difference before and after integration(P>0.05),but the RSD of the number and area of the integrated analytical units significantly decreased(P<0.05).Conclusion The MFSM method could reduce the analytical units of constituent herbal mate-rials while maintain the properties and variability from their original fingerprint.Thus,it could serve as a feasible and reliable tool to reduce difficulties in analyzing multi-compo-nents within CMMs and facilitating the evaluation of their quality.展开更多
[Objectives] To establish Thlaspi arvense L. HPLC fingerprints,to provide reference for quality evaluation Thlaspi arvense L.[Methods]HPLC chromatography was used,HPLC column Acclaim~ 120C_(18)( 250 mm × 3. 0 mm...[Objectives] To establish Thlaspi arvense L. HPLC fingerprints,to provide reference for quality evaluation Thlaspi arvense L.[Methods]HPLC chromatography was used,HPLC column Acclaim~ 120C_(18)( 250 mm × 3. 0 mm,5 μm),mobile phase of acetonitrile-0. 2% phosphoric acid aqueous solution gradient elution,flow rate of 0. 7 m L/min,column temperature of 30 ℃,detection wavelength of 320nm; the chromatographic fingerprint similarity evaluation software( Version 2004 A) was used for similarity evaluation and data processing on 10 origin Thlaspi arvense L. spectra,and the median method was used to generate control Thlaspi arvense L. fingerprint. [Results] The similarity of 10 origin Thlaspi arvense L. spectra was greater than 0. 90,19 common peaks were separated from different origin Thlaspi arvense L. and isovitexin,apigenin,luteolin and acacetin were identified. [Conclusions] The established HPLC fingerprint contained a lot of information and showed good specificity for Thlaspi arvense L.,which can provide a scientific basis for Thlaspi arvense L. quality evaluation system.展开更多
文摘For quality control purpose,an approach of combining chromatographic fingerprint of Huaijiao pill（HP）and simultaneous determination of its major bioactive components was developed using high performance liquid chromatography coupled with diode array detector（HPLC-DAD）.For fingerprint analysis,16 peaks were selected as the characteristic peaks to evaluate the similarities of different samples collected from different batches of three manufacturers.The similarities of 17 Huaijiao pill samples were beyond 0.966,indicating that samples from different batches and manufacturers were,to some extent,consistent.Additionally,simultaneous quantification of seven bioactive markers,namely sophoricoside,baicalin,naringin,genistein,rutin,quercetin and 5-O-methylvisammioside,in HP was performed to interpret the quality consistency.The validation of the proposed approach was acceptable,with the accuracy of 90.2%-106.9%in recovery test.The intra-day and inter-day precisions of the method were evaluated and the RSD values were less than 2.81%.The results from the quantitative data showed that the contents of six marker compounds（except for 5-O-methylvisammioside） were quite consistent between batches produced by one manufacturer and significantly distinctive among different manufacturers.The proposed approach was expected to be developed as a powerful tool for the quality control of HP.
基金supported the National Natural Science Foundation of China(Nos.20375050 and 20905080)National Key Technologies R&D Program of the 11th-five-year Plan(No.2006BAK03A08)Guangdong Provincial Department of Science and Technology(No.2009B010900021)
文摘Microwave-assisted extraction(MAE)was used for extraction of effective components of sarcandra glabra(Thunb.),and then chromatographic fingerprint of sarcandra glabra(Thunb.)was studied by high performance liquid chromatography/diode array detector(HPLC/DAD).The conditions of MAE were optimized by an orthogonal experiment,and then the authentication and validation of the chromatographic fingerprint were conducted.Nine peaks were identified as common peaks in the fingerprint chromatograms,and isofraxidin was considered as a reference compound and quantified.Relative standard deviations of retention time and peak area of each component were less than 3% and 8%,respectively.Similarity and difference analysis were conducted by use of PCA and relation coefficient.Twenty batches of sarcandra glabra(Thunb.)samples from two different producing areas could be classified into two different groups in the PCA model.The results showed that MAE-HPLC/DAD method was simple,efficient and stable for the study of complex chromatographic fingerprint of sarcandra glabra(Thunb.),which could provide more reliable and precise information for quality evaluation.
基金funded by Shandong Provincial Key Laboratory of Depositional Mineralization & Sedimentary Minerals (Project DMSM201009)Key Laboratory of Tectonics and Petroleum Resources (China University of Geosciences), Ministry of Education, China (Project TPR-2010-29)
文摘In this study, whole-oil gas chromatographic fingerprint analyses were performed on oils from the Es3^3 reservoir in the Liubei area of the Nanpu Sag. The gas chromatographic peaks of cyclic and branched alkanes with relatively high resolution from nCl0 to nC25 were selected to establish a database of whole-oil gas chromatographic peak height ratio fingerprints. Reservoir fluid connectivity was identified by using clustering analysis. This method can reflect the gas chromatography fingerprint information accurately and entirely, and avoid the one-sidedness of the star diagram method which only selects several fixed gas chromatographic peaks.
基金Foundation item： Projects（21275164, 21075138） supported by the National Natural Science Foundation of China
文摘A simple and facile gas chromatography-mass spectrometer （GC-MS） fingerprint of Su-He-Xiang-Wan （SHXW） was developed, the similarity analysis was conducted, and attribution of the major characteristic peaks was identified for SHXW quality control. GC-MS analysis was performed on a QP2010 instrument （Shimadzu, Japan） equipped with a capillary column of RTX-5MS. The column temperature was initiated at 50℃, held for 5 min, increased at the rate of 3 ℃/min to 120 ℃, held for 2 min, and then increased at the rate of 4 ℃/min to 220℃, held for 10 min. Helium carrier gas was used at a constant flow rate of 1.3 mL/min. Mass conditions were ionization voltage, 70 eV; injector temperature, 250℃; ion source temperature, 250 ℃; splitting ratio, 30：1; full scan mode in the 40-500 Da mass ranges with rate of 0.2 s per scan. Attribution of the major characteristic peaks was identified for SHXW by comparing the chemical standards, references of Chinese herbal medicines and the negative controls of prescription samples （NC） of SHXW. With the help of the temperature-programmed retention indices （PTRIs） used together with mass spectra and chemical standards, 25 major characteristic peaks have been identified. Nine volatile medicinal materials were identified in the prescription of SHXW by attributing to the 27 major characteristic peaks. The results demonstrate that the proposed method is a powerful approach to quality control of complex herbal medicines.
基金Natural Science Foundation of Hunan province(2022JJ30453 and 2024JJ6362)the Key Research and Development Program of Hunan Province(2022SK2014).
文摘Objective To facilitate the quality evaluation suitable for the unique characteristics of Chinese materia medica(CMM)by developing and implementing a novel approach known as the matching frequency statistical moment(MFSM)method.Methods This study established the MFSM method.To demonstrate its effectiveness,we applied this novel approach to analyze Danxi Granules(丹膝颗粒,DXG)and its constituent herbal materials.To begin with,the ultra-performance liquid chromatography(UPLC)was applied to obtain the chromatographic fingerprints of DXG and its constituent herbal materi-als.Next,the MFSM was leveraged to compress and integrate them into a new fingerprint with fewer analytical units.Then,we characterized the properties and variability of both the original and integrated fingerprints by calculating total quantum statistical moment(TQSM)parameters,information entropy and information amount,along with their relative standard deviation(RSD).Finally,we compared the TQSM parameters,information entropy and infor-mation amount,and their RSD between the traditional and novel fingerprints to validate the new analytical method.Results The chromatographic peaks of DXG and its 12 raw herbal materials were divided and integrated into peak families by the MFSM method.Before integration,the ranges of the peak number,three TQSM parameters,information entropy and information amount for each peak or peak family of UPLC fingerprints of DXG and its 12 raw herbal materials were 95.07−209.73,9390−183064μv·s,5.928−21.33 min,22.62−106.69 min^(2),4.230−6.539,and 50530−974186μv·s,respectively.After integration,the ranges of these parameters were 10.00−88.00,9390−183064μv·s,5.951−22.02 min,22.27−104.73 min^(2),2.223−5.277,and 38159−807200μv·s,respectively.Correspondingly,the RSD of all the aforementioned pa-rameters before integration were 2.12%−9.15%,6.04%−49.78%,1.15%−23.10%,3.97%−25.79%,1.49%−19.86%,and 6.64%−51.20%,respectively.However,after integration,they changed to 0.00%,6.04%−49.87%,1.73%−23.02%,3.84%−26.85%,1.17%−16.54%,and 6.40%−48.59%,respectively.The results demonstrated that in the newly integrated fingerprint,the analytical units of constituent herbal materials,information entropy and information amount were significantly reduced(P<0.05),while the TQSM parameters remained unchanged(P>0.05).Additionally,the RSD of the TQSM parameters,information entropy,and information amount didn’t show significant difference before and after integration(P>0.05),but the RSD of the number and area of the integrated analytical units significantly decreased(P<0.05).Conclusion The MFSM method could reduce the analytical units of constituent herbal mate-rials while maintain the properties and variability from their original fingerprint.Thus,it could serve as a feasible and reliable tool to reduce difficulties in analyzing multi-compo-nents within CMMs and facilitating the evaluation of their quality.
文摘[Objectives] To establish Thlaspi arvense L. HPLC fingerprints,to provide reference for quality evaluation Thlaspi arvense L.[Methods]HPLC chromatography was used,HPLC column Acclaim~ 120C_(18)( 250 mm × 3. 0 mm,5 μm),mobile phase of acetonitrile-0. 2% phosphoric acid aqueous solution gradient elution,flow rate of 0. 7 m L/min,column temperature of 30 ℃,detection wavelength of 320nm; the chromatographic fingerprint similarity evaluation software( Version 2004 A) was used for similarity evaluation and data processing on 10 origin Thlaspi arvense L. spectra,and the median method was used to generate control Thlaspi arvense L. fingerprint. [Results] The similarity of 10 origin Thlaspi arvense L. spectra was greater than 0. 90,19 common peaks were separated from different origin Thlaspi arvense L. and isovitexin,apigenin,luteolin and acacetin were identified. [Conclusions] The established HPLC fingerprint contained a lot of information and showed good specificity for Thlaspi arvense L.,which can provide a scientific basis for Thlaspi arvense L. quality evaluation system.
